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Methanol → 4-(5-Bromo-2,3-dihydrobenzofuran-2-yl)piperidine

HRID 1622247
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HRID 1622247 반응식
C(=O)([O-])[O-].[K+].[K+].[Br:7][C:8]1[CH:9]=[CH:10][C:11]2[O:15][CH:14]([CH:16]3[CH2:21][CH2:20][N:19](C(=O)C(F)(F)F)[CH2:18][CH2:17]3)[CH2:13][C:12]=2[CH:28]=1.CO.O>[Cl-].[Na+].O>[Br:7][C:8]1[CH:9]=[CH:10][C:11]2[O:15][CH:14]([CH:16]3[CH2:17][CH2:18][NH:19][CH2:20][CH2:21]3)[CH2:13][C:12]=2[CH:28]=1
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참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 11430Potassium CarbonateHCID 866748871-[4-(5-Bromo-2,3-dihydro-benzofuran-2-yl)-piperidin-1-yl]-2,2,2-trifluoro-ethanone

생성물 1

HCID 674691344-(5-Bromo-2,3-dihydrobenzofuran-2-yl)piperidine

시약·촉매·용매 1

HCID 57417360
Sodium chloride; water
용매

실험 절차

Potassium carbonate (10.17 g) is added to an ice-cooled mixture of 1-[4-(5-bromo-2,3-dihydro-benzofuran-2-yl)-piperidin-1-yl]-2,2,2-trifluoro-ethanone (4.64 g), methanol (120 mL), and water (30 mL). The reaction mixture is stirred over night at room temperature. Brine (150 mL) is added and the mixture is extracted with dichloromethane. The combined organic phases are dried over MgSO4 and concentrated in vacuo. The crude product is used for the next step without further purification. LC (method 2): tR=1.05 min; Mass spectrum (ESI+): m/z=282, 284 [M+H]+.

후처리

  1. temperaturecooled
  2. extractionthe mixture is extracted with dichloromethane
  3. dry with materialThe combined organic phases are dried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe crude product is used for the next step without further purification

출처 및 근거

ORD 기록
ord-ff506c79a105489fb15868d182e049bc
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08778926B2

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